反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 9.3 gm of 2,5-dichloro-4-hydroxyphenyl-glyoxal hydrate, 7.25 gm of 1-(3-amino-3-methylbutyl)-benzimidazole and 100 ml of alcohol was stirred for 3 hours at 40°-45° C. The resulting solution was subsequently cooled, admixed in portions with 8 gm of sodium borohydride, and the mixture was stirred for 3 hours at room temperature. After the addition of 100 ml of methanol for decomposition of the sodium borohydride, the mixture was allowed to stand for 10 hours, the solvent was distilled off under reduced pressure, the residue was dissolved in 200 ml of water, and the solution was acidified with concentrated hydrochloric acid. 9.5 gm of 1-(2,5-dichloro-4-hydroxyphenyl)-2-[4-(1-benzimidazolyl)-2-methyl-2-butylamino]-ethanol dihydrochloride×1H2O, m.p. 180°-183° C., of the formula ##STR29## were obtained. The yield was 50.4% of theory.
WORKUP
后处理
- temperatureThe resulting solution was subsequently cooled
- stirringthe mixture was stirred for 3 hours at room temperature
- waitto stand for 10 hours
- distillationthe solvent was distilled off under reduced pressure
- dissolutionthe residue was dissolved in 200 ml of water
- customwere obtained